超高效液相色谱法检测花生油中4种黄曲霉毒素的含量

Determination of aflatoxin content in peanut oil by UPLC

目的建立一种超高效液相色谱法测定花生油中4种黄曲霉毒素(B_1、B_2、G_1和G_2)含量的方法。方法花生油样品经甲醇-水提取后,静置2 min^3 min,过滤后稀释,用免疫亲和柱净化、浓缩。采用BEH C_(18)色谱柱(50 mm×2.1 mm,1.7μm),考察了不同流动相等度和梯度洗脱法,优化后的方法以甲醇-水溶液为流动相进行梯度洗脱,设定激发波长为360 nm、发射波长为450 nm进行检测。结果空白样品无干扰,4种黄曲霉毒素B_1、B_2、G_2在0.10μg/L^50.00μg/L,G_1在0.50μg/L^50.00μg/L时,线性关系良好,相关系数(r)均>0.999,最低检出限为0.04μg/kg^0.25μg/kg,相对标准偏差(RSD)为1.13%~8.82%,回收率为87.4%~104.6%。结论本方法简便、快速、准确,检出限低,干扰小,无需衍生,可用于粮油食品中黄曲霉毒素的检测。

Objective To develop a method for the determination of 4 kinds of aflatoxin（ B1,B2,G1,G2） in peanut oil by ultra performance liquid chromatography（ UPLC）. Methods The samples were extracted by the mixture of methanol- water;placed 2- 3 minutes in room temperature; then filtered,diluted,purified and concentrated with the immune affinity column.BEH（ 50 mm × 2. 1 mm,1. 7 μm） was used as the chromatographic column,the methanol- water was used as mobile phase for gradient elution. It was detected by fluorescence detector（ FLR） with excitation wavelength of 360 nm and emission wavelength of 450 nm. Results There was no interference in the blank sample. Good linearity was obtained when the mass concentration of aflatoxin B1,B2,G2 among 0. 10 μg / L- 50. 00 μg / L and aflatoxin G1 among 0. 50 μg / L- 50. 00 μg / L. The correlation coefficients（ r） were all 〉0. 999,the relative standard deviations（ RSDs） were among 1. 13%- 8. 82%,and the recoveries were among 87. 4%- 104. 6%. Conclusion This method is simple,rapid,precise,accurate,with low detection limit,little interference and little derivatization. Therefore,the method can be successfully used for the determination of aflatoxin in grain and oil.